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Formaldehyde → HCID 20426898, Verbindung

HRID 615700
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 615700
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9](=[O:22])[NH:10][CH:11]=[C:12]3[C:17]=2[NH:16][C:15]2[CH:18]=[CH:19][CH:20]=[CH:21][C:14]=2[S:13]3)=[CH:4][CH:3]=1.[OH-:23].[Na+].[CH2:25]=O>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9](=[O:22])[N:10]([CH2:25][OH:23])[CH:11]=[C:12]3[C:17]=2[NH:16][C:15]2[CH:18]=[CH:19][CH:20]=[CH:21][C:14]=2[S:13]3)=[CH:6][CH:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 712FormaldehydeHCID 14798Sodium HydroxideHCID 13051480HCID 13051480, Verbindung

Produkt 1

HCID 20426898HCID 20426898, VerbindungAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To 5.0 g. of 4-(4-chlorophenyl)-5H-pyrido[3,4-b][1,4]benzothiazin-3-(2H)-one (15.3 mmol.) in 50 ml. of dimethylformamide was added 30 ml. of a 5% sodium hydroxide solution (37.5 mmol.), and the resulting suspension was heated on a steam bath until a solution formed. To the solution was then added 50 ml. of a 36% formaldehyde solution (60.0 mmol.), and the resulting reaction mixture was heated until a yellow precipitate formed. The hot reaction mixture was filtered, and the precipitate was washed well with water and dried under high vacuum at room temperature to yield 4-(4-chlorophenyl)-2-(hydroxymethyl)-5H-pyrido[3,4-b][1,4]benzothiazin-3(2H)-one complexed with water (4:1) as a yellow powder (5.15 g.; 93% yield) having the structural formula, ##STR9## a melting point of greater than 300° C. and the following elemental analysis:

Aufarbeitung

  1. customformed
  2. additionTo the solution was then added 50 ml
  3. temperaturewas heated until a yellow precipitate
  4. customformed
  5. filtrationThe hot reaction mixture was filtered
  6. washthe precipitate was washed well with water
  7. customdried under high vacuum at room temperature

Quellen und Nachweise

ORD-Eintrag
ord-8369cc3a223b42048d98d97bc7c7c9d8
Quelldatensatz
uspto-grants-1985_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04500708

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